Quantitative determination of diterpenoid alkaloid Fuziline by hydrophilic interaction liquid chromatography (HILIC)–electrospray ionization mass spectrometry and its application to pharmacokinetic study in rats

Autor: Yunxi Zhong, Jianguo Sun, Guangji Wang, Fengyi Zhang, Jing-Han Liu, Ying Peng
Rok vydání: 2013
Předmět:
Zdroj: Journal of Chromatography B. :55-60
ISSN: 1570-0232
DOI: 10.1016/j.jchromb.2012.11.017
Popis: A rapid, sensitive and specific hydrophilic interaction liquid chromatography coupled to electrospray ionization mass spectrometric (HILIC-MS) method for the quantification of Fuziline (15α-Hydroxyneoline) in rat plasma was developed and validated. After liquid-liquid extraction with ethyl acetate, Fuziline and Guanfu base A (internal standard) were separated with HILIC Chrom Matrix HP amide column (5μm, 10cm×3.0mm I.D.) with isocratic elution at a flow-rate of 0.2mL/min. The analytes were detected by using an electrospray positive ionization mass spectrometry in the selected ion monitoring (SIM) mode. A good linear relationship was obtained in the concentration ranging from 1 to 1000ng/mL (R(2)=0.999) with the lower limit of quantification (LLOQ) at 1ng/mL and limit of detection (LOD) at 0.5ng/mL. The average recoveries of Fuziline in plasma at the concentrations of 2, 50, 1000ng/mL ranged from 68.2 to 69.9%. Intra- and inter-batch relative standard deviations ranged from 1.5 to 3.3% and 2.6 to 8.3%, respectively. Fuziline was stable under different sample storage and processing conditions except three-cycle freeze-thaw treatment at 2ng/mL. This method was successfully applied to the pharmacokinetic studies in Sprague-Dawley rats. The absolute bioavailability of Fuziline after oral administration 4mg/kg Fuziline in rats was 21.1±7.0%, with clearance rate at 1745.6±818.1mL/kg/h, and half-life at about 6.3±2.6h.
Databáze: OpenAIRE